CN109850951A - A method of iron oxide black is prepared using titanium white by product object - Google Patents
A method of iron oxide black is prepared using titanium white by product object Download PDFInfo
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- CN109850951A CN109850951A CN201910256339.0A CN201910256339A CN109850951A CN 109850951 A CN109850951 A CN 109850951A CN 201910256339 A CN201910256339 A CN 201910256339A CN 109850951 A CN109850951 A CN 109850951A
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Abstract
The present invention relates to iron oxide black technical field of producing, in particular to a kind of method for preparing iron oxide black using titanium white by product object, it using titanium white by product object as raw material, first pre-processes, then double purification, precipitating, iron oxide black is prepared, this method effectively removes impurity to titanium white by product object resource utilization, by easy method, industrial half solid waste is taken full advantage of, resource has been saved；In addition, simply and effectively controlling ferrous iron and ferric iron content, easy to operate, high-efficient, made iron oxide black quality is high.
Description
Technical field
It is the present invention relates to iron oxide black technical field of producing, in particular to a kind of to utilize the preparation oxidation of titanium white by product object
Iron black method.
Background technique
Titanium white by product object is byproduct caused by Titanium White Production By Sulfuric Acid Process, and every 1 ton of titanium dioxide of production will produce according to statistics
Raw 3.5~4 tons of by-products, a large amount of by-products are using traditional accumulation mode, and not only waste of resource, also pollutes environment, constitute serious
Security risk, for this purpose, very urgent to titanium white by product object resource utilization.
Iron oxide black scientific name ferroso-ferric oxide is a kind of magnetic black crystals of tool, is generally used for pigment or polishing machine,
It is also centainly applied on audio tape and communication electric appliance.Iron oxide black in the market is from magnetic iron ore deep processing, so mostly
And iron ore impurity content is varied, it is difficult to guarantee iron black purity, for this purpose, people start sight being transferred to chemistry side
On method production iron oxide black.
Main component is ferrous sulfate in titanium white by product object, secondly contains a small amount of impurity, is the ideal for producing iron oxide black
Raw material, the key of problem are how simple and effective removal impurity and to synthesize iron oxide black.In addition, ferrous iron and ferric iron exist in iron oxide black
Ratio is difficult to control in synthesis process, and gained iron oxide black is poor quality.Iron oxide black report is prepared not currently with titanium white by product object
Common, Chinese patent CN102659189A discloses a kind of pickle liquor preparation magnetic Fe3O4The method of nano-powder, by adding
Enter iron powder pickling of pretreatment liquid, oxidant is then added and accurately adjusts iron ion and ferrous ion content, adds alkali precipitation, wash
It washs, be drying to obtain iron oxide black.This method does not effectively remove other impurity first, and gained iron oxide black purity is not high, secondly, divalent
Iron and ferric iron content are difficult to control, and complicated for operation.
Summary of the invention
To solve the above problems, the present invention provides a kind of method for preparing iron oxide black using titanium white by product object, the party
Method simple process, accurately controls ferrous iron and ferric iron content.
Specifically, the invention discloses a kind of methods for preparing iron oxide black using titanium white by product object, which is characterized in that packet
Include following steps:
(1) pretreatment of titanium white by product object: preparing titanium white by product object solution, reduced iron powder is added, and additive is added, stirs
It mixes uniformly, stands, filtering；
(2) double purification: heating filtrate adds alkali to adjust pH to 2~3, stirring to 60~90 DEG C；It continues thereafter with plus alkali is adjusted
PH to 4.5~5.5 is stirred, filtering, the solution after obtaining double purification；
(3) precipitation reaction: being divided into solution A and two parts of solution B for purified solution, solution A be heated to 30~60 DEG C,
Alkali is added to adjust pH to 8~10, stirring；Solution B is heated to 70~90 DEG C, adds alkali to adjust pH to 6~8, is passed through enough air, stirs
It mixes；
(4) preparation of iron oxide black: A suspension and B suspension being mixed, stirred at 50~70 DEG C, filtered, washing,
Dry, grinding obtains iron oxide black particle.
Preferably, step (2) and the middle alkali being added of step (3) are ammonium hydroxide or sodium hydroxide.
Preferably, step (1):
The additive is the mixed solution of ammonium hydroxide and ammonium chloride, and wherein the mass ratio of ammonium hydroxide and ammonium chloride is 1:1~1:
3。
The titanium white by product object solution concentration is 50~150g/L；The dosage of iron powder is the 1~3% of titanium white by product object；Add
The dosage for adding agent is the 2~5% of titanium white by product object.
Step (1) time of repose does not have king-sized influence, preferably 10~30h to product preparation effect.
Preferably, step (2):
It is stirred after adding alkali to adjust pH to 2~3, preferably stirring 10~60min, more preferable 10~30min；Add alkali adjust pH to
It is stirred after 4.5~5.5, preferably stirring 10~60min, more preferable 10~30min.
Preferably, step (3):
Solution A stirs after adjusting pH, and mixing time does not have a king-sized influence to product preparation effect, preferably 10~
60min, more preferable 20~40min；It is stirred after solution B blowing air, mixing time does not have king-sized shadow to product preparation effect
It rings, preferably 10~100min, more preferable 40~60min.
Preferably, step (4):
A suspension and B suspension vol ratio are 0.45:1~0.5:1.
Heating stirring after A suspension and the mixing of B suspension, mixing time do not have king-sized shadow to product preparation effect
It rings, preferably 10~60min, more preferable 20~40min.
Further, 2~5% ammonium hydroxide of product quality is added in step (4) washing process.
Step (4) drying temperature is 50~80 DEG C.
Advantages of the present invention are as follows:
(1) present invention effectively removes impurity by easy method, takes full advantage of to titanium white by product object resource utilization
Industrial half solid waste, has saved resource；
(2) ferrous iron and ferric iron content simply and effectively are controlled, easy to operate, high-efficient, made iron oxide black product
Matter is high.
Detailed description of the invention
The following further describes the present invention with reference to the drawings
Fig. 1 is present invention process process
Specific embodiment
The present invention will be further described with reference to the examples below.Described embodiment and its result are merely to illustrate
The present invention, without the present invention described in detail in claims should will not be limited.
Embodiment 1
A method of iron oxide black being prepared using titanium white by product object, is included the following steps:
(1) pretreatment of titanium white by product object: a certain amount of titanium white by product object is taken to be configured to the solution of concentration 100g/L, molten
Quality is added in liquid and is the reduced iron powder of 1% titanium white by product object, and ammonium hydroxide and ammonium chloride that quality is 3% titanium white by product object is added
Mixed solution, the mass ratio of ammonium hydroxide and ammonium chloride is 1:1, stands 10h, filtering；
(2) double purification: heating filtrate adds ammonium hydroxide to adjust pH to 3 to 70 DEG C, stirs 20min；It continues thereafter with and adds ammonium hydroxide tune
PH to 5 is saved, 30min, filtering, the solution after obtaining double purification are stirred；
(3) precipitation reaction: being divided into solution A and two parts of solution B for purified solution, solution A is heated to 40 DEG C, ammonification
Water adjusts pH to 9, stirs 20min；Solution B is heated to 80 DEG C, adds ammonium hydroxide to adjust pH to 6, is passed through enough air, is stirred
40min；
(4) preparation of iron oxide black: A suspension and B suspension are mixed according to volume ratio 0.48:1, stirred at 60 DEG C
20min is filtered, and is washed, dry, and grinding obtains iron oxide black particle.
Gained iron oxide black product purity is high, content of impurities are lower than 0.5%.
Embodiment 2
A method of iron oxide black being prepared using titanium white by product object, is included the following steps:
(1) pretreatment of titanium white by product object: a certain amount of titanium white by product object is taken to be configured to the solution of concentration 150g/L, molten
Quality is added in liquid and is the reduced iron powder of 3% titanium white by product object, and ammonium hydroxide and ammonium chloride that quality is 5% titanium white by product object is added
Mixed solution, the mass ratio of ammonium hydroxide and ammonium chloride is 1:2, stands 30h, filtering；
(2) double purification: for heating filtrate to 90 DEG C, adding sodium hydroxide adjusts pH to 2.5, stirs 30min；It continues thereafter with and adds
Sodium hydroxide adjusts pH to 4.5, stirs 20min, filtering, the solution after obtaining double purification；
(3) precipitation reaction: purified solution is divided into solution A and two parts of solution B, solution A is heated to 30 DEG C, adds hydrogen
Sodium oxide molybdena adjusts pH to 10, stirs 30min；Solution B is heated to 90 DEG C, adding sodium hydroxide adjusts pH to 7, is passed through enough air
Stir 60min；
(4) preparation of iron oxide black: A suspension and B suspension are mixed according to volume ratio 0.45:1, stirred at 70 DEG C
30min is filtered, and is washed, dry, and grinding obtains iron oxide black particle.
Gained iron oxide black product purity is high, content of impurities are lower than 0.5%.
Embodiment 3
A method of iron oxide black being prepared using titanium white by product object, is included the following steps:
(1) pretreatment of titanium white by product object: a certain amount of titanium white by product object is taken to be configured to the solution of concentration 50g/L, molten
Quality is added in liquid and is the reduced iron powder of 2% titanium white by product object, and ammonium hydroxide and ammonium chloride that quality is 2% titanium white by product object is added
Mixed solution, the mass ratio of ammonium hydroxide and ammonium chloride is 1:3, stands 20h, filtering；
(2) double purification: heating filtrate adds ammonium hydroxide to adjust pH to 2 to 60 DEG C, stirs 10min；It continues thereafter with and adds ammonium hydroxide tune
PH to 5 is saved, 10min, filtering, the solution after obtaining double purification are stirred；
(3) precipitation reaction: being divided into solution A and two parts of solution B for purified solution, solution A is heated to 60 DEG C, ammonification
Water adjusts pH to 8, stirs 40min；Solution B is heated to 70 DEG C, adds ammonium hydroxide to adjust pH to 8, is passed through enough air, is stirred
50min；
(4) preparation of iron oxide black: A suspension and B suspension are mixed according to volume ratio 0.5:1, stirred at 50 DEG C
40min is filtered, and is washed, dry, and grinding obtains iron oxide black particle.
Gained iron oxide black product purity is high, content of impurities are lower than 0.5%.
Claims (10)
1. a kind of method for preparing iron oxide black using titanium white by product object, which comprises the steps of:
(1) pretreatment of titanium white by product object: preparing titanium white by product object solution, reduced iron powder is added, and additive is added, and stirring is equal
It is even, it stands, filtering；
(2) double purification: heating filtrate adds alkali to adjust pH to 2~3, stirring to 60~90 DEG C；Continue thereafter with plus alkali adjust pH to
4.5~5.5, it stirs, filtering, the solution after obtaining double purification；
(3) precipitation reaction: purified solution is divided into solution A and two parts of solution B, solution A is heated to 30~60 DEG C, adds alkali
Adjust pH to 8~10, stirring；Solution B is heated to 70~90 DEG C, adds alkali to adjust pH to 6~8, is passed through enough air, is stirred；
(4) preparation of iron oxide black: A suspension and B suspension being mixed, stirred at 50~70 DEG C, filtered, and washed, dry,
Grinding, obtains iron oxide black particle.
2. the method according to claim 1, wherein the alkali being added in step (2) and step (3) is ammonium hydroxide or hydrogen
Sodium oxide molybdena.
3. the method according to claim 1, wherein step (1) additive is the mixed of ammonium hydroxide and ammonium chloride
Solution is closed, wherein the mass ratio of ammonium hydroxide and ammonium chloride is 1:1~1:3.
4. the method according to claim 1, wherein step (1) titanium white by product object solution concentration is 50~150g/
L；The dosage of iron powder is the 1~3% of titanium white by product object；The dosage of additive is the 2~5% of titanium white by product object.
5. the method according to claim 1, wherein step (1) time of repose is 10~30h.
6. preferably being stirred the method according to claim 1, wherein step (2) plus alkali stir after adjusting pH to 2~3
Mix 10~60min, more preferable 10~30min；It is stirred after adding alkali to adjust pH to 4.5~5.5, preferably 10~60min of stirring, it is more excellent
Select 10~30min.
7. the method according to claim 1, wherein step (3) solution A adjust pH after stir, preferably 10~
60min, more preferable 20~40min；It is stirred after solution B blowing air, preferably 10~100min, more preferable 40~60min.
8. the method according to claim 1, wherein step (4) A suspension and B suspension vol ratio are 0.45:
1~0.5:1.
9. being stirred the method according to claim 1, wherein being heated after step (4) A suspension and the mixing of B suspension
It mixes, preferably 10~60min, more preferable 20~40min.
10. the method according to claim 1, wherein product quality 2~5% is added in step (4) washing process
Ammonium hydroxide；Drying temperature is 50~80 DEG C.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649588A (en) * | 2012-04-18 | 2012-08-29 | 四川大学 | Method for producing iron oxide red by using ferrous sulfate as titanium dioxide byproduct |
| CN104071850A (en) * | 2013-03-25 | 2014-10-01 | 北京三聚环保新材料股份有限公司 | Preparation method for iron oxide black |
| CN104386764A (en) * | 2014-11-20 | 2015-03-04 | 周淑华 | Method for producing iron oxide black by acid waste water in titanium-dioxide industry |
| CN105439211A (en) * | 2015-12-17 | 2016-03-30 | 江苏省常熟环通实业有限公司 | Energy-saving environmental-protection production method for iron oxide black pigment |
| CN107673410A (en) * | 2017-10-19 | 2018-02-09 | 兰州城市学院 | The method that nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid |
-
2019
- 2019-04-01 CN CN201910256339.0A patent/CN109850951B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649588A (en) * | 2012-04-18 | 2012-08-29 | 四川大学 | Method for producing iron oxide red by using ferrous sulfate as titanium dioxide byproduct |
| CN104071850A (en) * | 2013-03-25 | 2014-10-01 | 北京三聚环保新材料股份有限公司 | Preparation method for iron oxide black |
| CN104386764A (en) * | 2014-11-20 | 2015-03-04 | 周淑华 | Method for producing iron oxide black by acid waste water in titanium-dioxide industry |
| CN105439211A (en) * | 2015-12-17 | 2016-03-30 | 江苏省常熟环通实业有限公司 | Energy-saving environmental-protection production method for iron oxide black pigment |
| CN107673410A (en) * | 2017-10-19 | 2018-02-09 | 兰州城市学院 | The method that nano ferriferrous oxide is prepared using industrial ferrous contained waste liquid |
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